関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Acetylpiperazine | HCID 83795 | — |
| 反応物 | 2-Chloro-4'-fluoroacetophenone | HCID 120248 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-Acetyl-4-(4-fluorophenylcarbonylmethyl)-piperazine hydrochloride | HCID 9904442 | 99.9% |
反応手順
A suspension of 1-acetylpiperazine (0.627 g), 2-chloro-4′-fluoroacetophenone (0.844 g), and potassium hydrogen carbonate (0.735 g) in acetonitrile (12 ml) was stirred at ambient temperature for 3 days. After removal of the solid by filtration, the filtrate was evaporated under reduced pressure to give a residue, which was chromatographed on silica gel (100 ml) eluting with 0%-5% methanol in dichloromethane. The objective compound of the free form was taken up into ethyl acetate (2 ml) and to the solution was added a solution of hydrogen chloride in ethyl acetate (4N, 2 ml). The resulting precipitate was collected by filtration, washed with diisopropyl ether, and dried in vacuo to give 1-acetyl-4-(4-fluorophenylcarbonylmethyl)-piperazine hydrochloride (1.47 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710043B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-3e6c4ebfd1b54107b7d522df8874cc92 |
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| 出典メモ | uspto-grants-2004_03 |
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